HRID422558

反应详情

EQUATION

反应方程式

HRID 422558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 4-methyl-3-(1-(1,1,1-trifluoroprop-2-en-2-yl)phthalazin-6-yl)benzoate (200 mg, 537 μmol) in methanol (3000 μl) was added palladium (10 wt. % on activated carbon; 22.9 mg, 215 μmol) and hydrogenated (double-walled balloon pressure) at room temperature for 20 h, during which LC-MS indicated complete conversion. The reaction was filtered via a pad of Celite®, and the filtrate was concentrated in vacuo and purified by CombiFlash (20% to 80% EtOAc/Hexanes) to afford methyl 4-methyl-3-(1-(1,1,1-trifluoropropan-2-yl)phthalazin-6-yl)benzoate (91.1 mg, 45.3% yield) as a golden yellow foam. MS (ES+): 375.2 (M+H)+.

WORKUP

后处理

  1. filtrationThe reaction was filtered via a pad of Celite®
  2. concentrationthe filtrate was concentrated in vacuo
  3. custompurified by CombiFlash (20% to 80% EtOAc/Hexanes)